气相色谱法测定菝葜中薯蓣皂苷元含量

目的 建立菝葜中薯蓣皂苷元的含量测定方法。方法 程序升温气相色谱法，CP Sil 5CB熔融石英毛细管柱，FID检测器。结果薯蓣皂苷元在0．20～5.0μg范围内具有良好的线性关系，r=0．9998，测定方法平均回收率为97．20％。结论 本方法有较高的灵敏度和回收率，可用于菝葜中薯蓣皂苷元的含量测定。     

贵州产菝葜类8种药用植物中薯蓣皂苷元的分析

目的 采用TLC、RP-HPLC法分析贵州产菝葜属及肖菝葜属8种常用药用植物中的指标性成分薯蓣皂苷元.方法 TLC法采用硅胶G板,以环己烷-乙酸乙酯(4:1)为展开剂.RP-HPLC的色谱条件为依利特Hypersil ODS2色谱柱(250 mm ×4.6 mm,5 μm),流动相为甲醇-0.2%磷酸(76:24),流速1.0 mL·min~(-1),检测波长203 nm,柱温30℃,薯蓣皂苷元理论板数不低于4×10~3.结果 薄层鉴别中仅有短梗菝葜、黑叶菝葜及小叶菝葜含有薯蓣皂苷元.薯蓣皂苷元0.0105～2.105 μg与峰面积呈良好的线性关系;平均加样回收率为100.4%(RSD=1.85%,n=9).黑叶菝葜的薯蓣皂苷元含量最高,为0.15%,土茯苓、柔毛菝葜、托柄菝葜、短柱肖菝葜中均未检测到薯蓣皂苷元.结论 所用TLC法及RP-HPLC法简单易行、专属性强、准确度高、重复性好,可作为菝葜类药材内在质量的控制方法.     

气相色谱法测定菝葜中薯蓣皂苷元含量

目的　建立菝葜中薯蓣皂苷元的含量测定方法。方法　程序升温气相色谱法 ,CPSil 5CB熔融石英毛细管柱 ,FID检测器。结果　薯蓣皂苷元在 0 2 0～ 5 0 μg范围内具有良好的线性关系 ,r=0 9998,测定方法平均回收率为 97 2 0 %。 结论　本方法有较高的灵敏度和回收率 ,可用于菝葜中薯蓣皂苷元的含量测定。     

菝葜、土茯苓和土萆薜的薄层色谱鉴别

目的建立一种方法对药材性状相似的三种药材菝葜、土茯苓和土草醉进行定性鉴别。方法应用TLC对菝葜、土茯苓和土草薜水解前后的化学成分进行分析比较。结果实验表明菝葜、土茯苓和土草醉均含有β-谷甾醇。菝葜含有薯蓣皂苷元，可能含有菝葜皂苷元；土茯苓和土草醉不合薯蓣皂苷元或量微，可能含有菝葜皂苷元。结论三者既含有相同的化学成分，又有不同的化学成分，可以区别。     

菝葜药用植物的资源调查及品质分析

目的:探讨菝葜的资源品质与生态环境的关系。方法:选取全国有代表性的菝葜主产区进行资源调查,采集样品和生态环境资料;采用薄层色谱法鉴别不同产地菝葜中的白藜芦醇、落新妇苷和黄杞苷,采用反相高效液相色谱法测定薯蓣皂苷元的含量。结果:不同产地菝葜药材中白藜芦醇、落新妇苷和黄杞苷的斑点强弱差异较大,薯蓣皂苷元的含量差异明显。结论:菝葜药用植物的品质与其生态环境之间具有一定的相关性。     

高效液相-蒸发光散射检测器法测定知母中菝葜皂苷元含量

目的：采用高效液相-蒸发光散射检测器（HPIC-EISD）法测定知母中菝葜皂苷元的含量。方法：ODS-C8柱，流动相为甲醇-水，梯度洗脱。因菝葜皂苷元为一甾体皂苷元，无紫外特征吸收，选择了通用型检测器-蒸发光散射检测器（ELSD）。结果：菝葜皂苷元在0.12～4.0μg范围内具良好的线性关系，r=0．9998，平均回收率为98．3％。结论：本方法有较高的灵敏度和回收率，可用于知母中菝葜皂苷元的含量测定。     

不同炮制方法对知母体外抗菌活性的影响

目的探讨不同炮制方法的知母提取物及其活性物质菝葜皂苷元的体外抗菌活性。方法采用试管连续稀释法对痢疾杆菌、大肠杆菌、金黄色葡萄球菌和铜绿假单胞菌进行体外抑菌试验。结果 菝葜皂苷元对痢疾杆菌、大肠杆菌、金黄色葡萄球菌和铜绿假单胞菌有较强的抑制作用；不同炮制方法的知母提取物有不同程度的抑制作用，其中以盐麸制法抗菌效价最高，其上述4种致病菌最低抑菌浓度（MIC）分别为12．5，25．0，25．0，50．0μg／mL。结论盐麸制法的知母其体外抗菌活性最强，菝葜皂苷元对知母的抗菌作用特异性较强。     

高效液相色谱法测定乳宁片中菝葜皂苷元含量

目的建立测定乳宁片中菝葜皂苷元含量的高效液相色谱（HPLC）法。方法采用AgilentSBC18柱（250mm×4．6mm,5μm）,以甲醇-水（91：9）为流动相,流速为0．8mL／min,应用蒸发光散射检测器检测,漂移管温度为80℃,气体流速为2．0mL／min。结果菝葜皂苷元进样量在0．7536～6．7824μg范围内与峰面积积分值对数呈对数线性关系（r：0．9984）,平均回收率为99．22％,RSD=0．87％（n=6）。结论该法操作简便,专属性强,检测结果准确可靠,可用于乳宁片的质量控制。     

双波长薄层扫描法测定菝葜皂苷元含量

目的：建立双波长薄层扫描法测定知母药材及知母制剂中菝葜皂苷元含量的方法。方法：知母药材的乙醇提取液为2mol·L-1盐酸水解,用氯仿萃取,薄层条件：硅胶G薄层板,展开剂：正己烷-乙酸乙酯（1：1）,显色剂：8％香草酸无水乙醇溶;70％硫酸溶液（1：5）,参比波长600nm,检测波长445nm。结果：菝葜皂苷元在1～3μg范围内呈线性（γ=0.9998）,平均回收率99．5％（RSD=1．99％）。结论：方法简便,可靠。     

菝葜、土茯苓和土萆薢的薄层色谱鉴别

目的 建立一种方法对药材性状相似的三种药材菝葜、土茯苓和土萆薢进行定性鉴别.方法 应用TLC对菝葜、土茯苓和土萆薢水解前后的化学成分进行分析比较.结果 实验表明菝葜、土茯苓和土草薢均含有β-谷甾醇.菝葜含有薯蓣皂苷元,可能含有菝葜皂苷元;土茯苓和土草薢不含薯蓣皂苷元或量微,可能含有菝葜皂苷元.结论 三者既含有相同的化学成分,又有不同的化学成分,可以区别.     

Trichloroethylene. I. Carcinogenicity of trichloroethylene.

Trichloroethylene (TCE) as an industrial pollutant may damage human health and can be considered as carcinogen. TCE has been detected in the environment and in various human organs, e.g., liver, kidney and brain etc. There are histological alterations such as depletion of glycogen and hydropic degeneration in the liver, however, other signs of TCE effects can be found in various organs as well. TCE and its metabolites, e.g., trichlorethanol, trichloro-acetic acid and epoxides were recently identified as strong mutagens in Ames mutagenicity test inducing frameshift and base-substitution mutations. TCE induced predominantly hepatocellular carcinoma after long term administration in mice. In these animals, kidneys and liver were supposed to be primary target organs with low epoxy-hydrolase activity. A high level of mitotic gene conversion (or gene rearrangement) was indicated by the metabolism of TCE after repeated administration. Purified TCE by was a weak mutagen in the presence of S9 microsomal fraction of rats and as a consequence, the carcinogenic activity was low in the kidney of rats. However, a dose related increase of Leydig cell tumors was found in male rats.     

Trichloroethylene. II. Mechanism of carcinogenicity of trichloroethylene.

The cancer inducing effect of trichloroethylene (TCE) was studied by various methods. DNA complexing activity and apoptosis inhibition were found to be the key elements of the carcinogenicity of TCE and its metabolites. The ability of TCE to interact with DNA was low, but its incorporation into the RNA and DNA of the brain, testis, pancreas, kidney, liver, lung and spleen, cannot be excluded. Exposure to TCE and its metabolites provides a selective growth advantage to spontaneously occurring mutations in some K- and H-ras oncogenes (as non specific results of secondary DNA or RNA damage). The amount of DNA-TCE adducts was higher in mouse hepatocytes than in rat hepatocytes. These differences may explain the species difference in carcinogenicity of TCE, which was dose dependent (due to metabolism) in mice but independent in rats. The blood level kinetics of TCE confirmed the faster metabolic rate in mice, including peroxisome proliferation and induction in hepatocytes. Dichloroacetic- and trichloroacetic acid were found to be hepatic carcinogens in mice, and the specificity depends on peroxisome proliferation induction. Possibly, TCE and related compounds down regulated apoptosis in mouse liver, and the reduced ability to remove initiated cells by apoptosis could be responsible for liver cancer induction by TCE.     

Studies in antifertility agents. 11. Secosteroids. 5. Synthesis of 9,11-secoestradiol.

9,11-Secoestradiol (9) and 11-hydroxy-9,11-secoestradiol (12) have been synthesized starting from 17-acetoxyestradiol 3-methyl ether (1) and found to possess significant antifertility activity in rats. 3-Methoxy-9,11-seco-9-oxo-17beta-acetoxyestra-1,3,5(10)-trien-11-oic acid (2), prepared by CrO3 oxidation of 1, on hydrogenolysis gave methyl 17beta-hydroxy-3-methoxy-9,11-secoestra-1,3,5(10)-triene-11-carboxylate (3). The 17-O-THP derivative of 3 was treated with LiAlH4 to give 17beta-(O-tetrahydropyranyl)-3-methoxy-11-hydroxy-9,11-secoestra-1,3,5(10)-triene (5). The 11-O-mesylate of 5 on LiAlH4 reduction followed by mild acid treatment and demethylation under alkaline conditions gave 9. LiAlH4 reduction of 3 gave 9,11-seco-11-hydroxyestradiol 3-methyl ether (11) which on demethylation gave 9,11-seco-11-hydroxyestradiol (12).     

Metabolism of benzothiazole. I. Identification of ring-cleavage products.

1. The metabolic fate of benzothiazole in guinea pig has been investigated following i.p. administration at a dose of 30 mg/kg. 2. Five ring-cleavage products were identified in urinary extracts by g.l.c.-mass spectra. By reference to authentic compounds the three major metabolites were shown to be 2-methylmercaptoaniline (I), 2-methylsulphinylaniline (II) and 2-methylsulphonylaniline (III). On the basis of the mass spectrometric evidence the remaining two metabolites were postulated to be 2-methylsulphinylphenylhydroxylamine (IV) and 2-methylsulphonylphenylhydroxylamine (V). 3. I, II and III were present in conjugated and unconjugated forms; IV and V were identified only after hydrolysis with sulphatase.